Green-black vat-dye.



Ph. 1)., chemist, a citizen of the Empire of Main, (irermany have invented certain new acctylamitlophenylthioglycollic ortho car- UNiTEn srii rss Parana chines.-

ALBRECHT SCHMIDT, OF HQGHS'P-ON-TllE-MATX, GERMANY, ASSTGNOR TO FARBWERKE VORM. MEISTER LUOIUS & BltUNl'NG, Oi" llOCIIST-ON-THl LMAlN, (-EERMANY, A CORPO- RATION OF GERMAN Y.

GREEN-BLACK VAT-IDYE.

Specification of Letters Patent.

Patented Nov. 26, 1907.

To a-ll whom it may concern:

Be it known that I, ALBRECHT Seuum'r,

Germany, and residing at lliichst-on-thcand useful Improvements in Making a New Greenish-Black Vat- Dyestulf, of which the following is a SQOC-lllCnLlOn.

I have found a new greenish black vat dyestui'f having the formula:

NH.,(L)(7H;, :;;C: C:C C::: C,H3M)NH, being a black powder, insoluble in water, alkalihydrates, dilute acids, alcohol, ether, benzene, soluble in concentrated sulfuric acid with a greenish dark blue color, yielding with alkaline hydrosulfite solution a yellowish-greenish vat from which wool and cotton are dyed greenish black tintsv This vat dyestutf may be obtained, for instance, by heatboxylic acid of the type coon cm swrncoon Nu, or its acidyl derivatives, for instance,

coon (m on, s-cinoooruo Nnoocu i with allmlihydratcs and by oxidizing the leuco bodies isolated from the melt, paraamidooxythionaphthone carboxylic acid or para-amidooxythionaphthene.

The parent material, for instance, the paraboxylic acid coon on our, scu.,coou(o NIIotLCH, (I) may be obtained as follows; 110 gr. of acetaminoanthramlic acid CUHII:Nll :NllU II ,t)=t;: l :t

are dissolved in 50 of sodium hydrate and water. After adding 150 c.c. ol' conccntrated lr ulrochloric acid and ice the solution is diazotized with 35 oi sodium mtrue.

'lhis diayo solution is allowed to run at about I 7U -75 17. into an aqueous solutionot' lobar.

of potassium xanthogenate and 200 gr. of

sodium carbonate; the filtered solution is treated with 75 gr. of (-ldoracetic acid, dissolved in about 90 er. of caustic soda and water and heated to ebulliticn for some hours. After filtration the solution is )recipitated with dilute hydrochloric acid, w ion the acetamidophenylthioglycollicorthocar boxylic acid is precipitated as a brownish owder. The melt is obtained, for instance, as follows: 30 parts of this acid are introduced at about 100 C. in tSO parts of caustic soda liquefied with about 30 parts or more of water. The temperature is gradually raised while stirring to about l7t)1S-)t) (1., till the melt becomes brittle.

The operation may also occur by heating with less alkali or under pressure. The product of condensation may be isolated in various ways: Thus, for instance, the stirring may occur, with little water and the sodium salt of para-amidooxytliionaphtlicne-carboxylic acid thus separated and soluble with dilliculty inv alkalihydratc, readily soluble in water,- is filtered from the excess of the alkalihydrate solution.

The product of condensation of p ara-amidooxythionaphthene-carboxylic acid may also be obtained from the aqueous solution of the strongly cooled melt by directly acidifying with acetic acid, when it is precipitated as a crystalline powder. It is soluble in an excess of hydrochloric acid in the beat, as well as in a solution of sodium carbonate; on boiling, *arbonic acid is evolved, and the liquid solidifies to a magna of munone vellow needles of para-ainidooxythionaphthoue. it is soluble in other with a strong ellow-greenish fluorescence and is colorless 1n soda-lyc and mineral acids.

The oxidation of the store-described leuco bodies may be carried out in the following manner: 30 parts by weight of the above mentioned carl ox \'lic acid or of para-amid oxythionaphtbone are dissolved in the heat with ISO parts of smla-lye and 200 parts of water, the solution being then treated with air at about 'Ttt so i. till no further amidooxythiouaphthone carboxylic acid or amidooxythionaphthene can be traced in the lil trate. The operation may also occur by .boxylic acid obtained oxidizing in a neutral or alkalicarbonatealkaline suspension instead of in a much diwith limited quantities of Water. The oxidation may also occur with ferric salts,

potassium ferri-cyanid and the like in neutral or feebly alkaline solution.

The dyestufl separated in greenish black flakes by one or the other method is isolated from the mother-lye by filtration and may be urified from small inter-mixtures by boiling with alcohol. When dry,it is a black powder, insoluble in water, alkalihydrates, dilute acids, alcohol, ether, benzene, soluble in concentrated sulfuric acid with a greenish dark blue color, yielding with alkaline hydrosulfite solution a yellowish greenish vat from which wool and cotton are dyed greenish black tints.

Having now described my lnvention, what I claim is:

As product, the greenish black vat dyestuii' having the formula:

being insoluble in water, alkalihydrates, dilute acids, alcohol, ether, benzene, soluble 1n concentrated sulfuric acid with a greenish dark blue color, yielding with alkaline hydrosulfite solution a yellowish-greenish vat from which wool and cotton are dyed greenish-black tints.

In testimony, that I claim the foregoing as my invention, I have signed my name in presence of two subscribing witnesses.

ALBRECHT SCHMIDT.

Witnesses:

JEAN GRUND, CARL GRUND. 

